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Clean production method of hesperidin

A clean production, hesperidin technology, applied in chemical instruments and methods, sugar derivatives, sugar derivatives, etc., can solve problems such as the problem of hesperidin not being solved, and achieve increased farmers' income, energy saving, and obvious economic benefits. and social benefits

Inactive Publication Date: 2012-01-11
四川天予植物药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] None of the above studies has solved the existing problems in the production of hesperidin

Method used

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  • Clean production method of hesperidin

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Experimental program
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Effect test

Embodiment 1

[0015] Get 100g of Citrus aurantium powder that has been crushed through a 10-mesh sieve into a conical flask, add 500ml of 60% methanol solution (v / v) containing 0.7% potassium hydroxide, soak for 3 hours, filter to get the supernatant, and then add 400ml of 60% methanol solution (v / v) containing 0.7% potassium hydroxide, soak and extract for 3 hours, 3 hours, 3 hours and 2 hours respectively, filter, combine five extracts, add hydrochloric acid to adjust the pH to 4 while stirring . Let stand for 2 hours, filter with suction, wash the crystals with a small amount of 60% methanol and water, and dry at 80°C to obtain 29.3g of the product. The purity was 98.3% by HPLC, and the content by external standard method was 95.3%.

Embodiment 2

[0017] Get the Fructus Citrus Fructus Citrus powder 100g that has been pulverized through 10 mesh sieves in the leakage tube, add 85% ethanol solution (v / v) 300ml that contains 1.5% sodium hydroxide, soak for 3 hours, begin to leak, leak 1500ml altogether, The seepage was collected and stirred while adding hydrochloric acid to adjust the pH to 7. Stand still for 2 hours, filter with suction, wash the crystals with a small amount of 85% ethanol and water, and dry at 80°C to obtain 28.5g of the product. The purity was 98.7% by HPLC, and the content by external standard method was 95.5%.

Embodiment 3

[0019] Get the Fructus Citrus Fructus Citriifolia powder 100g that has been crushed through a 10 mesh sieve into the leakage tube, add 70% methanol solution (v / v) 300ml containing 0.8% sodium hydroxide, soak for 3 hours, start to leak, and leak 2500ml altogether, Collect the seepage while stirring and add acetic acid to adjust the pH to 6. Let it stand for 2 hours, filter with suction, wash the crystals with a small amount of 70% methanol and water, and dry at 80°C to obtain 30.3g of the product. The purity was 98.1% by HPLC, and the content by external standard method was 95.2%.

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Abstract

The invention discloses a clean production method of hesperidin. By adding proper amount of an alkaline organic solvent methanol (ethanol) to carrying out extraction on fruits of immature citron, and then using a method of precipitation by adding acid, hesperidin is precipitated. The principle of the method comprises the followings: carrying out extraction by using a method that the ring opening of hesperidin in the alkaline solvent can generate a water soluble and water containing organic solvent, then using a method of acidifying to let hesperidin be subject to ring-closure crystallization to generate the hesperidin with extremely low solubility in the water and water containing methanol (ethanol), and purifying with a method of non-crystallizable impurities to obtain the high quality hesperidin. According to the invention, the obtained product has good property and high yield, and has the primary crystal content of more than 95 %; by recovering the solvents, the pollution is avoided; and the method is suitable for large-scale industrialized production. However, in the prior art of alkali extraction and acid precipitation, a large number of sewage is generated, which pollutes environment greatly, and the products of the prior art has low content and bad property.

Description

technical field [0001] The present invention designs a method for cleanly producing hesperidin by using the fallen citrus fruit of aurantium aurantium as a raw material. Background technique [0002] Citrus aurantium is the fruit drop formed by natural selection during the growth of citrus. It is a raw material of Chinese herbal medicine. However, due to the small amount of clinical use, a large amount of Citrus aurantium is mainly used for the production of hesperidin. Hesperidin has the functions of increasing the resistance of capillaries, maintaining the normal permeability of blood vessels, inhibiting the increase of blood cholesterol and preventing arteriosclerosis. It is widely used as medical drugs, health products and food additives. Diosmin, which is semi-synthesized using hesperidin as a raw material, is commonly used in Europe to treat various symptoms related to venous lymphatic insufficiency and various symptoms related to acute hemorrhoids. Bureau approved fo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/07C07H1/08
Inventor 许育海严绍华李威李选民
Owner 四川天予植物药业有限公司
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